JPS6333563A - Production of pt-ni alloy for sputtering - Google Patents
Production of pt-ni alloy for sputteringInfo
- Publication number
- JPS6333563A JPS6333563A JP17494586A JP17494586A JPS6333563A JP S6333563 A JPS6333563 A JP S6333563A JP 17494586 A JP17494586 A JP 17494586A JP 17494586 A JP17494586 A JP 17494586A JP S6333563 A JPS6333563 A JP S6333563A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- mold
- ingot
- water
- sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 229910000990 Ni alloy Inorganic materials 0.000 title claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 26
- 229910002845 Pt–Ni Inorganic materials 0.000 claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 8
- 238000005336 cracking Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、スパッタリング用Ｐｔ−Ｎｉ合金ターゲット
の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for manufacturing a Pt--Ni alloy target for sputtering.
（従来の技術）
Ｐｔ−Ｎｉ合金は、非常に硬く、脆い材料である為、従
来、半導体用スパッタリングターゲット材料として使用
するものは、Ｐｔ−Ｎｉ合金又はｐｔ粉末とＮｉ粉末を
使用した粉末冶金法による焼結材料で作られていた。(Prior art) Since Pt-Ni alloy is a very hard and brittle material, conventionally used as sputtering target material for semiconductors is Pt-Ni alloy or powder metallurgy method using PT powder and Ni powder. Made of sintered material.
（発明が解決しようとする問題点）
然し乍ら、前記焼結材料では緻密度が１００％のものは
作りにくい為、材料中に吸蔵する不純ガスが問題となる
。その場合、材料の純度の低下のみならず、スパッタリ
ング中の異常放電などの現象が起こり、形成される膜の
特性に多大な影響を与えていた。(Problems to be Solved by the Invention) However, since it is difficult to make the sintered material with 100% density, impurity gas occluded in the material becomes a problem. In this case, not only the purity of the material decreases, but also phenomena such as abnormal discharge during sputtering occur, which greatly affects the characteristics of the formed film.
その為、吸蔵する不純ガスの少ない真空溶解及び塑性加
工によるＰ ｔ −Ｎ ｉ合金ターゲットが要求されて
いた。Therefore, there has been a demand for a Pt-Ni alloy target that is subjected to vacuum melting and plastic working with less occluded impurity gas.
ところでＰｔ−Ｎｉ合金は、Ｎｉｌの増加に伴い硬さが
大きく変化し、第７図に示す如＜３０ｗｔ％付近で最大
となる。Ｐｔ−Ｎｉ合金で１５〜４０ｗ ｔ％のＮｉを
含む合金の溶湯を鋳型に鋳造すると、鋳型の温度上昇に
より結晶粒が粗大化しく特に湯口付近）、脆い材料とな
る為、塑性加工を行うと粒界割れが発生し、しかも熱処
理時ヒートクラック等が発生し、従ってＰｔ−Ｎｉ合金
ターゲットを作ることができなかった。By the way, the hardness of the Pt-Ni alloy changes greatly as the Ni content increases, and reaches its maximum at around <30 wt% as shown in FIG. When a molten Pt-Ni alloy containing 15 to 40 wt% Ni is cast into a mold, the temperature of the mold increases and the crystal grains become coarse (especially near the sprue), resulting in a brittle material. Grain boundary cracking occurred, and heat cracks etc. occurred during heat treatment, and therefore a Pt--Ni alloy target could not be produced.
（発明の目的）
本発明は、上記問題点を解決すべくなされたものであり
、塑性加工時粒界割れを抑止でき、しかも熱処理時ヒー
トクラック等の発生を防止できるスパッタリング用Ｐ
ｔ −Ｎ ｉ合金ターゲ、７トの製造方法を提供するこ
とを目的とするものである。(Object of the Invention) The present invention has been made to solve the above problems, and provides a P for sputtering that can suppress grain boundary cracking during plastic working and also prevent the occurrence of heat cracks during heat treatment.
It is an object of the present invention to provide a method for manufacturing a t-Ni alloy target.
（問題点を解決するだめの手段）
上記問題点を解決するための本発明のスパッタリング用
Ｐ ｔ −Ｎ ｉ合金ターゲットの製造方法は、Ｐｔ−
Ｎｉ合金を溶解し、これを熱容量の大きな鋳造鋳型又は
水冷鋳型にて鋳造し、鋳型の温度上昇を抑えてＰｔ−Ｎ
ｉ合金インゴットを作り、然る後所要の形状に塑性加工
することを特徴とするものである。(Means for Solving the Problems) The method for manufacturing a Pt-Ni alloy target for sputtering of the present invention to solve the above-mentioned problems is as follows:
Pt-N is melted by melting the Ni alloy and casting it in a casting mold with a large heat capacity or a water-cooled mold to suppress the rise in temperature of the mold.
This method is characterized by producing an i-alloy ingot and then plastically working it into a desired shape.
（作用）
上記の如く本発明の製造方法では、溶解したＰｔ−Ｎｉ
合金を熱容量の大きな鋳造鋳型又は水冷鋳型にて鋳造し
、鋳型の温度上昇を抑えてＰｔ−Ｎｉ合金インゴットを
作るので、この作られたＰｔ−Ｎｉ合金インゴットの結
晶粒は均一化され且つ微細化されている。従って、塑性
加工での粒界割れの発生が防止され、Ｐｔ−Ｎｉ合金イ
ンゴットを強加工することができ、熱処理時のヒートク
ラックの発生も防止することができる。(Function) As described above, in the production method of the present invention, dissolved Pt-Ni
The alloy is cast in a casting mold with a large heat capacity or a water-cooled mold, and the temperature rise of the mold is suppressed to produce a Pt-Ni alloy ingot, so the crystal grains of the produced Pt-Ni alloy ingot are made uniform and fine. has been done. Therefore, the occurrence of intergranular cracks during plastic working is prevented, the Pt-Ni alloy ingot can be strongly worked, and the occurrence of heat cracks during heat treatment can also be prevented.
（実施例）
本発明のスパッタリング用Ｐ ｔ −Ｎ ｉ合金ターゲ
ットの製造方法の一実施例を従来例と共に説明する。(Example) An example of the method for manufacturing a Pt-Ni alloy target for sputtering according to the present invention will be described together with a conventional example.
先ず本発明の一実施例について説明する。ｐｔ−Ｎ ｉ
３９．２ｗｔ％合金を溶解し、これを熱容量の大きな
鋳造鋳型、本例では第１図に示す寸法の二分割のＣｕ鋳
型１に鋳造し、鋳型１の温度上昇を１５０度迄抑えて第
２図に示すＰ ｔ −Ｎ ｉ ３９．２ｗｔ％合金のイ
ンゴット２を作った。このインゴット２は一部破断して
示したように結晶粒が均一化され且つ微細化されていた
。然してこのインゴット２をクロス圧延し、幅２９５
ｎ、長さ１８０ｆｌ、厚さ６．ｆ）ｍｎのプレートに成
形した処、粒界割れが極めて小さかった。尚、前記鋳型
１の体積はインゴット２の体積の１０．６倍で、鋳型１
の熱容量は著しく大きいものである。First, one embodiment of the present invention will be described. pt-Ni
39.2wt% alloy is melted and cast into a casting mold with a large heat capacity, in this example, a two-part Cu mold 1 having the dimensions shown in Fig. 1. An ingot 2 of a Pt-Ni 39.2wt% alloy shown in the figure was made. As shown in the partially broken ingot 2, the crystal grains were uniform and fine. This ingot 2 was then cross-rolled to a width of 295 mm.
n, length 180fl, thickness 6. f) When molded into a mn plate, grain boundary cracking was extremely small. The volume of the mold 1 is 10.6 times the volume of the ingot 2, and the volume of the mold 1 is 10.6 times that of the ingot 2.
The heat capacity of is extremely large.
また前記インゴット２を加工率６５％で厚さ１７．０鶴
から６ 、 Ｏｍｎまで圧延加工した処、中心部まで完
全に塑性変形していた。これをＮｚ Ｈｚ雰囲気中で
８００℃、４０分間熱処理した後、水中急冷したがヒー
トクラックの発生は無かった。Further, when the ingot 2 was rolled at a processing rate of 65% from a thickness of 17.0 mm to a thickness of 6.0 mm, the center part was completely plastically deformed. This was heat-treated at 800° C. for 40 minutes in a Nz Hz atmosphere and then rapidly cooled in water, but no heat cracks occurred.
次に従来例について説明する。Ｐ ｔ −Ｎ ｉ３２．
９％合金を溶解し、これを第５図に示す寸法の二分割の
Ｃｕ鋳型３に鋳造し、鋳型３の温度上昇を抑えずに第６
図に示すＰ ｔ −Ｎ ｉ３２．９％合金のインゴット
４を作った。このインゴット４は一部破断して示したよ
うに特に湯口付近の部分が結晶粒の粗大化が見られた。Next, a conventional example will be explained. Pt-Ni32.
A 9% alloy was melted and cast into a two-part Cu mold 3 having the dimensions shown in FIG.
An ingot 4 of a Pt-Ni 32.9% alloy shown in the figure was made. As shown in the partially broken ingot 4, coarsening of crystal grains was observed especially in the area near the sprue.
然してこのインゴット４をクロス圧延し、幅２００鶴、
長さ２０ＯＮ、厚さ８．Ｏｎのプレートに成形した処、
粒界割れが極めて大きかった。尚、前記鋳型３の体積は
インゴット２の体積の３．２倍で、鋳型３の熱容量は小
さいものである。This ingot 4 was then cross-rolled to a width of 200 mm.
Length 20ON, thickness 8. The part formed on the On plate,
Grain boundary cracking was extremely large. The volume of the mold 3 is 3.2 times the volume of the ingot 2, and the heat capacity of the mold 3 is small.
また前記インゴット４を加工率３０％で厚さ１７０から
１２鰭まで圧延加工した処、厚さ方向の中間部の塑性変
形は小さかった。これをＮｚ Ｈｇ雰囲気中で８００
℃、４０分間熱処理した後、水中急冷した処ヒートクラ
ックが著しく発生した。Further, when the ingot 4 was rolled to a thickness of 170 to 12 fins at a processing rate of 30%, plastic deformation in the intermediate portion in the thickness direction was small. This was heated to 800°C in a Nz Hg atmosphere.
After heat treatment at ℃ for 40 minutes, significant heat cracking occurred during quenching in water.
このように従来の製造方法ではインゴット４に結晶粒の
粗大化が見られ、クロス圧延した際粒界割れが極めて大
きいのに対し、本発明の製造方法ではインゴット１の結
晶粒が均一微細化され、クロス圧延した際粒界割れが極
めて小さいので、インゴットの塑性加工性が優れている
ことが判る。In this way, in the conventional manufacturing method, coarsening of the crystal grains is observed in the ingot 4, and extremely large grain boundary cracks occur when cross-rolled, whereas in the manufacturing method of the present invention, the crystal grains in the ingot 1 are uniformly refined. It can be seen that the ingot has excellent plastic workability because intergranular cracks are extremely small when cross-rolled.
また従来の製造方法では圧延加工後の熱処理でヒートク
ラックが生じたが、本発明の製造方法では加工率の高い
圧延加工後の熱処理でもヒートクランクの発生が無く、
耐熱性に優れたＰ ｔ −Ｎ ｉ合金ターゲットが得ら
れることが判る。In addition, in the conventional manufacturing method, heat cracks occurred during the heat treatment after rolling, but in the manufacturing method of the present invention, no heat cracks occur even during the heat treatment after rolling, which has a high processing rate.
It can be seen that a Pt-Ni alloy target with excellent heat resistance can be obtained.
尚、本発明の製造方法で使用する熱容量の大きな鋳型１
の変形例としては第３図ａに示す如く湯口付近のボリュ
ームを大きくした鋳型５や第３図すに示す如く下端より
上端に向かって次第に太くなるようにテーパを付した鋳
型６がある。また熱容量の大きな鋳型の代わりに、第４
図ａに示す如（上部外面に波形の水冷管７．７′を配管
した水冷鋳型８や第４図すに示す如く上部に上下に平行
な折り返し水冷管９．９′を挿通配管した水冷鋳型１０
を用いても良いものである。In addition, mold 1 with a large heat capacity used in the manufacturing method of the present invention
As a modification, there is a mold 5 which has a larger volume near the sprue as shown in FIG. 3a, and a mold 6 which is tapered so that it gradually becomes thicker from the lower end toward the upper end as shown in FIG. Also, instead of a mold with a large heat capacity, a fourth mold is used.
As shown in Figure a (a water-cooled mold 8 with corrugated water-cooled pipes 7, 7' installed on the outer surface of the upper part, and a water-cooled mold 8 with vertically parallel folded water-cooled pipes 9,9' inserted in the upper part as shown in Figure 4). 10
It is also possible to use
（発明の効果）
以上の説明で判るように本発明のスパッタリング用Ｐｔ
−Ｎｉ合金ターゲットの製造方法によれば、結晶粒の均
一微細なインゴットを鋳造できて、塑性加工時粒界割れ
を抑止でき、しかも熱処理時ヒートクラック等の発生の
無い品質の良好なＰｔ−Ｎｉ合金ターゲットが得られる
という効果がある。(Effect of the invention) As can be seen from the above explanation, the Pt for sputtering of the present invention
- According to the method for manufacturing a Ni alloy target, it is possible to cast an ingot with uniform and fine crystal grains, suppress intergranular cracking during plastic working, and produce high-quality Pt-Ni that does not cause heat cracks during heat treatment. This has the effect that an alloy target can be obtained.
第１図は本発明の製造方法で用いた熱容量の大きな鋳型
を示す斜視図、第２図は第１図の鋳型により作られたイ
ンゴットの断面マクル組織を示す図、第３図ａ、ｂは夫
々熱容量の大きな鋳型の変形例を示す斜視図、第４図ａ
、ｂは夫々水冷鋳型の例を示す斜視図、第５図は従来の
製造方法で用いた鋳型を示す斜視図、第６図は第５図の
鋳型により作られたインゴットの断面マクロＭｉ織を示
す図、第７図はＰｔ−Ｎｉ合金の硬さを示すグラフであ
る。
出願人 田中貴金属工業株式会社
５．６・・・俯を
第５図 第６図
第７図
Ｐｔ 重！ ’／。 ＮＬFigure 1 is a perspective view showing a mold with a large heat capacity used in the manufacturing method of the present invention, Figure 2 is a diagram showing the cross-sectional macrostructure of the ingot made by the mold of Figure 1, and Figures 3a and b are A perspective view showing a modified example of a mold with a large heat capacity, FIG. 4a
, b are perspective views showing examples of water-cooled molds, FIG. 5 is a perspective view showing a mold used in the conventional manufacturing method, and FIG. The figure shown in FIG. 7 is a graph showing the hardness of Pt-Ni alloy. Applicant: Tanaka Kikinzoku Kogyo Co., Ltd. 5.6...Downward view Fig. 5 Fig. 6 Fig. 7 Pt Heavy! '/. N.L.
Claims (1)
鋳型又は水冷鋳型にて鋳造し、鋳型の温度上昇を抑えて
Ｐｔ−Ｎｉ合金インゴットを作り、然る後所要の形状に
塑性加工することを特徴とするスパッタリング用Ｐｔ−
Ｎｉ合金ターゲットの製造方法。Pt-Ni alloy is melted and cast in a casting mold with a large heat capacity or a water-cooled mold, a Pt-Ni alloy ingot is produced by suppressing the rise in temperature of the mold, and then plastically worked into the desired shape. Features of Pt- for sputtering
A method for manufacturing a Ni alloy target.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17494586A JPS6333563A (en) | 1986-07-25 | 1986-07-25 | Production of pt-ni alloy for sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17494586A JPS6333563A (en) | 1986-07-25 | 1986-07-25 | Production of pt-ni alloy for sputtering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6333563A true JPS6333563A (en) | 1988-02-13 |
Family
ID=15987478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17494586A Pending JPS6333563A (en) | 1986-07-25 | 1986-07-25 | Production of pt-ni alloy for sputtering |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6333563A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0544024A (en) * | 1991-03-19 | 1993-02-23 | Mitsubishi Materials Corp | Production of thin cylindrical stock for vapor deposition |
| WO2002077306A1 (en) * | 2001-03-21 | 2002-10-03 | Vishay Intertechnology, Inc. | Method of suppressing the oxidation characteristics of nickel |
| US6723280B2 (en) | 2001-04-02 | 2004-04-20 | Vishay Vitramon Incorporated | Method of suppressing the oxidation characteristics of nickel |
| EP1721997A1 (en) * | 2004-03-01 | 2006-11-15 | Nippon Mining & Metals Co., Ltd. | Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY |
| CN104018128A (en) * | 2014-05-29 | 2014-09-03 | 贵研铂业股份有限公司 | Nickel-platinum alloy sputtering target material and preparation method thereof |
| JP2015025176A (en) * | 2013-07-26 | 2015-02-05 | 三菱マテリアル株式会社 | Ni OR Ni ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD OF THE SAME |
| CN104726829A (en) * | 2013-12-18 | 2015-06-24 | 有研亿金新材料股份有限公司 | High purity NiPt alloy target material and preparation method thereof |
| US9249497B2 (en) | 2010-03-19 | 2016-02-02 | Jx Nippon Mining & Metals Corporation | Ni alloy sputtering target, Ni alloy thin film and Ni silicide film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61124566A (en) * | 1984-11-19 | 1986-06-12 | Mitsubishi Metal Corp | Production of al-si alloy target plate material for sputtering |
-
1986
- 1986-07-25 JP JP17494586A patent/JPS6333563A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61124566A (en) * | 1984-11-19 | 1986-06-12 | Mitsubishi Metal Corp | Production of al-si alloy target plate material for sputtering |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0544024A (en) * | 1991-03-19 | 1993-02-23 | Mitsubishi Materials Corp | Production of thin cylindrical stock for vapor deposition |
| WO2002077306A1 (en) * | 2001-03-21 | 2002-10-03 | Vishay Intertechnology, Inc. | Method of suppressing the oxidation characteristics of nickel |
| US7208218B2 (en) | 2001-03-21 | 2007-04-24 | Vishay Vitramon Incorporated | Method of suppressing the oxidation characteristics of nickel |
| US6723280B2 (en) | 2001-04-02 | 2004-04-20 | Vishay Vitramon Incorporated | Method of suppressing the oxidation characteristics of nickel |
| EP1721997A1 (en) * | 2004-03-01 | 2006-11-15 | Nippon Mining & Metals Co., Ltd. | Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY |
| EP1721997A4 (en) * | 2004-03-01 | 2009-11-11 | Nippon Mining Co | Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY |
| US7959782B2 (en) | 2004-03-01 | 2011-06-14 | Jx Nippon Mining & Metals Corporation | Method of manufacturing a Ni-Pt alloy |
| EP2468906A1 (en) | 2004-03-01 | 2012-06-27 | JX Nippon Mining & Metals Corporation | Method of manufacturing a Ni-Pt alloy |
| US9249497B2 (en) | 2010-03-19 | 2016-02-02 | Jx Nippon Mining & Metals Corporation | Ni alloy sputtering target, Ni alloy thin film and Ni silicide film |
| JP2015025176A (en) * | 2013-07-26 | 2015-02-05 | 三菱マテリアル株式会社 | Ni OR Ni ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD OF THE SAME |
| CN104726829A (en) * | 2013-12-18 | 2015-06-24 | 有研亿金新材料股份有限公司 | High purity NiPt alloy target material and preparation method thereof |
| CN104018128A (en) * | 2014-05-29 | 2014-09-03 | 贵研铂业股份有限公司 | Nickel-platinum alloy sputtering target material and preparation method thereof |
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